• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention is depicting a chemical separation of phorphorus ore. Phosphorus ore, especially calcareous and clacareous-sillicious phosphorus ore can be effectively converted into several products through chemical separation, which consists of two stages, namely ore pulp reaction and solution regeneration. In the first stage, phosphorus ore is disolved by mixed ammonium salts solvent, but the valence minerals, such as fluoride apatite and quartz don't take part in the reaction and retain their solid state. Thus phosphorus concentrate can be obtained through the separation, the by-products such as the filtrate and gases can be utilized in the solution regeneration. After ammoniation, sulfurization, carbonization and alkalization of the filtrate, the Ca2+, Mg2+, Fe3+, Al2+, M2+ ions in it will gradually come out and turn into products, the regenerated solution obtained can be used again and again, thus forming a complete enclosed circulation process.
    公开号:SU1516006A3
    申请号:SU864027339
    申请日:1986-04-01
    公开日:1989-10-15
    发明作者:Венксинг Лю
    申请人:Шаанкси Кемикал Фертилайзер Индастриал Компани (Фирма)；Кемира Ой (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to the technology of enrichment of phosphate raw materials and can be used in chemical industry in the production of fertilizers.
    The aim of the invention is to reduce the loss of phosphorus.
    Example I. Phosphorus-containing ore from Cha Dian, Shaanxi Province, China.
    The chemical composition of the original ore,%: phosphorus pentoxide 20.47; calcium oxide 38.08; magnesium oxide 5.47; iron oxide 1.82; alumina 1.71; silica 10.47; oxide mfgants 2.41.
    The implementation of the method.
    Processing of ore sludge: took 1000 g of the original powdered ore 100W and 6500 g of the solution of amine salts
    at a concentration of 18% (at a weight ratio of ammonium chloride and ammonium nitrate of 4.3: 1), which made it possible to prepare ore sludge, which was loaded into a vessel with agitation, increased the temperature to and pressure to 2 kg / cm and kept under these conditions for 60 min, then the reaction mixture was filtered to obtain a phosphorus concentrate as a filter cake, and the filtrate and gaseous ammonia and carbon dioxide released during the reaction were sent to the treatment at the stage of solution regeneration.
    Regeneration solution.
    Ammokieatsi. The filtrate discharged from the ore sludge reaction stages was pumped into a vessel for replenishing ammonia with ammonia, increased
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    temperature up to 50 ° C, Ca (C10) "was added in an amount, 4 which was 100% of the amount theoretically necessary for the oxidation of ferrous ion, kept under these conditions for 10 minutes, the ammonia solution in iodine was added again to bring pH was 7-8; the reaction was carried out for 30 minutes; the mixture was filtered, hydrates of ferric oxides and aluminum were in the form of a filter cake, for subsequent use, and the filtrate was sent for vulcanization.
    Vulcanization. The filtrate, removed from stage ai {monization, was pumped into the vulcanization vessel, the stirrer was turned on, the temperature was raised to, sulphide am 1oni was added in an amount equal to 105% of the amount theoretically necessary for the divalent manganese ion, the reaction mixture was heated to temanium containing products then
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    the filtrate, after adding hydrochloric acid and adjusting the pH to 7, can be reused as a regenerated solution.
    The main products obtained during the experiment are presented in the table.
    Loss of phosphorus was 0.58%. According to the prototype, the loss of phosphorus was 2.4%.
    Example 2: Take phosphorus ore from Hi Jai Yang, Shahxi Province, China.
    The chemical composition of the original ore,%: phosphorus pentoxide 17.25; calcium oxide 43.22; magnesium oxide 7.46; ferric oxide 0.82; alumina oxide 20 0.39; silica 3,44; manganese oxide 3.27.
    The method was carried out as follows.
    Processing of ore sludge. For
    thirty
    25 min and filtered, the preparation of ore sludge preparation was 1000 g
    the original powdered ore 100W and 6700 g of a solution of mixed amine salts (with a weight ratio of ammonium chloride and ammonium nitrate 4: 1) with a concentration of 17.4%, after which the mixture was loaded into a vessel, the stirrer was turned on and the temperature was raised to 105 C. 6 hours under normal pressure, then the reaction mixture was filtered to give phosphorus concentrate as the remaining filter cake, while the filtrate, as well as ammonia and carbon dioxide gas, which released manganese sulfide in the form of a filter cake, which can be processed to obtain manganese-containing products and regenerate ammonium feed, and the filtrate goes to the carbonation step.
    Carbonization. The filtrate, withdrawing from the vulcanization stage, was pumped into the carbonization vessel, the stirrer was turned on, the temperature was raised to and the continuous flow of gaseous ammonia and carbon dioxide was started, from the ore sludge treatment stage
    magnesium-containing products whereas
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    the filtrate, after adding hydrochloric acid and adjusting the pH to 7, can be reused as a regenerated solution.
    The main products obtained during the experiment are presented in the table.
    Loss of phosphorus was 0.58%. According to the prototype, the loss of phosphorus was 2.4%.
    Example 2: Take phosphorus ore from Hi Jai Yang, Shahxi Province, China.
    The chemical composition of the original ore,%: phosphorus pentoxide 17.25; calcium oxide 43.22; magnesium oxide 7.46; ferric oxide 0.82; alumina 0.39; silica 3,44; manganese oxide 3.27.
    The method was carried out as follows.
    Processing of ore sludge. For
    bonization Such a reaction can be carried out; during the reaction, it can be sent in combination with ore processing for processing at the stage of regenerated oil. After carbonization, the reaction mixture was grafted and crystalline calcium carbonate was obtained as a filter cake, and the filtrate was sent to the alkalisation stage.
    Alkalinization The filtrate removed from the carbonization stage was pumped into the alkaline vessel, the stirrer was turned on, the temperature was raised to 50 ° C, and the amount of concentrated liquid ammoniac was added in the quantity required. To adjust the pH to 12, keep the reaction mixture for 30 minutes, filter and isolate magnesium oxide hydrate as a filter cake, which can be further processed to obtain
    im rastor
    Regeneration pacTBOpai. Vulcanization. The filtrate removed from the ore slurry reaction stage was pumped into the curing vessel, the stirrer was turned on, the temperature was raised to 55 ° C, and ammonium sulfide was added to the mixture in an amount of 105% of that required for divalent manganese ions. The reaction time was 25 minutes. After that, the reaction mixture
    filtered, the filter residue, which is manganese sulphide, can be sent for further processing to obtain manganese-containing products and a regenerator
    ammonium sulphide, and the filtrate was transported to the carbonation stage.
    Carbonization. The filtrate obtained from the vulcanization stage was pumped into the carbonization vessel, the stirrer was switched on, and the temperature was raised to and the continuous flow of gaseous ammonia and carbon dioxide discharged from the ore slurry reaction stage started. This reaction could be carried out in combination with ore sludge treatment. After that, the reaction mixture was filtered to obtain a residue on a filter containing crystalline calcium carbonate, while the filtrate was sent to the alkalisation stage.
    Alkalinization The filtrate removed from the carbonation stage was pumped into the alkaline vessel, the stirrer was turned on, the temperature was raised to 50 ° C, and then 25% ammonia solution was added in the amount necessary to bring the pH of the mixture to 12 (extreme point). The total reaction time was 30 minutes. Far, the reaction mixture was filtered, and the remaining magnesium oxide hydrate could be used for further processing to obtain magnesium-containing products, while the filtrate, after adjusting its pH to 7-8, could be reused as a regenerated solution.
    The results of the experiment are presented in the table.
    Example 3: Take phosphorus ore from Chi Jai Yang, Shahxi Province, China.
    The chemical composition of the original ore,%: phosphorus pentoxide 17.25; oxide. calcium 43.22; magnesium oxide 7.46; ferric oxide 0.82; alumina 0.93; silica 3,44; bivalent manganese oxide 3.23.
    The method is carried out as follows.
    Processing of ore sludge. To prepare the ore sludge, 1000 g of the initial powder ore 100 W and 6500 g of a solution of mixed amine salts with a concentration of 16.50% were taken (Lree weight ratio of ammonium sluoride and
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    ammonium nitrate 4: 1), after which the mixture was loaded into the reaction vessel, the stirrer was switched on, the temperature was raised to 140 ° C and the pressure was increased to 2 kg / cm, the reaction was carried out for 4 h, then the reaction mixture was filtered to obtain phosphorus as a filter residue concentrate, and the filtrate, together with gaseous ammonia and carbon dioxide, which were released during this reaction, were sent for further processing at the stage of solution regeneration.
    Regeneration solution.
    Vulcanization. The filtrate, which was removed from the ore sludge treatment stage, was sent to a vulcanization vessel, the stirrer was switched on, the temperature was raised to 55 ° C, and ammonia sulphide was added (in an amount that was 105% of that required for divalent manganese ions). After 25 minutes of reaction, the reaction mixture was filtered, the filter residue was sent for further processing to obtain manganese-containing products and regenerate ammonium sulfide, while the filtrate was sent to the carbonization step.
    Carbonization. The filtrate withdrawn from the vulcanization stage was pumped into the carbonization vessel, the stirrer was switched on and the temperature was raised to 40 ° C, after which continuous flow of ammonia gas and carbon dioxide gas was started, which was removed from the ore sludge treatment stage for carbonization.
    This reaction could be carried out in combination with the processing of ore sludge. Then, the reaction mixture was solvated, obtaining crystalline calcium carbonate as a filter residue, while the filtrate was sent to alkalization.
    Alkalinization The filtrate withdrawn from the carbonization stage was pumped into the alkaline vessel, the stirrer was turned on, the temperature was raised to, a 25% ammonia solution was added in an amount necessary to bring the pH to 12 (extreme point). The total reaction time is 30 minutes. Then the reaction mixture was filtered to obtain magnesium oxide hydrate as a filter residue, which can be sent for further processing to obtain magnesium-containing products, and the filtrate, after adding nitric acid to it and bringing the pI to 7-9, can be further used as regenerated solution.
    The results of the experiment are presented in the table.
    Example 4: Take phosphorus ore from Hi Jai Yang, Shaanxi Province, China.
    The chemical composition of the original ore,%: phosphorus pentoxide 17.25; calcium oxide 43.22; ferric oxide 0.82; alumina 0.39; silica 3,44; bivalent manganese oxide. 3,27.
    The method was carried out as follows.
    Reactions involving ore sludge. To prepare the ore sludge, 1000 g of raw powder ore 100W and 6000 g of a solution of mixed amine salts with a concentration of 16% were taken (at a weight ratio of ammonium chloride and ammonium nitrate 4: 1), after which this mixture was pumped into the reaction vessel, the stirrer was turned on, the temperature was raised to 180 ° C, and the pressure to 6 kg / cm. Under these conditions, peaKUiiro was carried out for more than 80 minutes, the mixture was poured to produce phosphorus concentrate as a filter, while gaseous ammonia and carbon dioxide released during the reaction were sent for further processing to the stage of solution regeneration.
    Regenerated solution.
    Vulcanization. The filtrate removed from the ore slurry reaction stage was pumped into the vulcanization vessel, the stirrer was turned on, and the temperatures were raised to 55 ° C, after which ammonium sulphide was added in an amount that was 105% of the amount of divalent manganese . The reaction time was 25 minutes, after which the reaction mixture was filtered, the filtrate residue was used for further processing in order to study manganese-containing products and also for the regeneration of ammonium sulfide, while the filtrate was directed to carbonation.
    Carbonization. The filtrate from the vulcanization stage was pumped into the vessel dd.
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    carbonization, turn on the stirrer, raise the temperature to 40 ° C and start. purging through the liquid continuous streams of gaseous ammonia and carbon dioxide, which were removed from the reaction stage with the participation of ore sludge. This reaction could be carried out in combination with the processing of ore sludge. Next, the reaction mixture was filtered to obtain crystalline calcium carbonate as a filter residue, while the filtrate was sent to the alkalizing step.
    Alkalinization The filtrate from the carbonization stage was pumped into an alkaline vessel, the stirrer was switched on, the temperature was raised to and a 25% ammonia solution was added in an amount necessary to bring the pH to 12 (final point), then the reaction was filtered for 30 minutes and the reaction mixture was filtered. The remaining magnesium oxide hydrate in the form of a filter residue can be used for further processing to produce magnesium-containing products, while the filtrate, after adding nitric acid to it and adjusting its pH to 7-8, can be used as a regenerated solution.
    The results of the experiment are presented in the table.
    An example. Pick up phosphorus ore from Da Tang, Gizhu Province, China.
    The chemical composition of the original ore,%: phosphorus pentoxide 21.86; calcium oxide 43.00; magnesium oxide 8.70; ferric oxide 0.5; alumina 0.57; silica 3.71.
    The method was carried out as follows.
    Processing of ore sludge. For the preparation of ore sludge, 1000 g of raw powder ore 100W and 6600 g of a solution of mixed amine salts with a concentration of 17% (at a weight ratio of ammonium chloride, ammonium nitrate and secondary ammonium phosphate 3.6: 1: 0.1) were taken and loaded into the reaction mixture the vessel, the stirrer was turned on, and the temperature was raised to g, and the pressure to 6 kg / cm. Reaction time 60 min | After that, the reaction mixture 1filtered getting in the form of a filter residue
    9151
    phosphate concentrate, while the filtrate and ammonia gas and carbon dioxide, which were separated during the reaction, were sent for further processing at the stage of solution regeneration.
    Regeneration solution.
    Carbonization. The filtrate from the ore slurry reaction stage was pumped into the carbonization vessel, the stirrer was turned on, the temperature was raised to 40 ° C, and ammonia gas and carbon dioxide, which separated during the processing of the ore slurry, were blown through the liquid. This reaction can be carried out in combination with the processing of ore sludge. Next, the reaction mixture was filtered, having obtained crystalline calcium carbonate as a filtered residue, while the filtrate was sent for alkalization.
    Alkalinization The filtrate from the carbonization stage was pumped into the alkalization vessel, the stirrer was switched on, the temperature was raised to 25% ammonia solution was added to bring the pH to 12 (final point), the reaction was filtered for 30 minutes and the reaction mixture was filtered. The remaining magnesium oxide hydrate in the form of a filter residue can be used for further processing to obtain magnesium-containing products, while the filtrate, after adding nitric acid to it, can be used as a regenerated solution to adjust the pH.
    The results of the experiment are presented in the table.
    Example 6. Phosphorus-containing ore was taken from Mo Ping, Gizhu Province, China.
    The chemical composition of the original ore,%: phosphorus pentrxide 30,69; calcium oxide 48.41; magnesium oxide 2.82; ferric oxide 0.79; alumina 0.29.
    The method was carried out as follows.
    Processing of ore sludge. For the preparation of ore sludge, 1000 g of raw, 80W powdered ore and 6000 g of a solution of mixed amine salts with a concentration of 14.5% (with a weight ratio of ammonium chloride and ammonium nitrate. 5.6: 1) were taken, after which the mixture was loaded into a reaction vessel.
    00610
    Turn on the stirrer and raise the temperature to. The reaction was carried out under normal pressure for 24 hours. After that, the reaction mixture was filtered to obtain a phosphorus concentrate in the filter residue, while the filtrate and ammonia gas and carbon dioxide were directed for further processing at the stage of solution regeneration.
    Regeneration solution. The filtrate from the reaction stage with the participation of ore sludge was pumped into a vessel for carbonization, the stirrer was turned on, and the temperature was raised to, and then continuous flows of gaseous ammonia and carbon dioxide started to flow through the liquid.
    0 stages of processing ore slurry for carbonization. This reaction can be carried out in combination with the processing of ore sludge. After that, the reaction mixture was filtered, getting in the form
    5 of the filter residue is crystalline calcium carbonate, while the filtrate can then be reused as a regenerated solution. ,
    0 The results of the experiment are presented in the table.
    Example. Pick up phosphorus ore from Mo Ping, Gui-Zhu Province, China.
    X1-1mic composition of the original ore,%: phosphorus pentoxide 30,69; calcium oxide 48,4li; magnesium oxide 2.82;
    ferric oxide 0.79; alumina 0.29.
    Q The method was carried out in the following way.
    Processing of ore sludge. For the preparation of ore sludge, 1000 g of the initial powdered ore was taken.
    with 80W and 6000 g of a solution of mixed amine salts with a concentration of 14.5 (with a weight ratio of ammonium chloride and ammonium nitrate of 5.6: 1), after which the mixture was sent to a reaction vessel,
    0 the stirrer was turned on and the temperature was raised to 140 ° C. The reaction was carried out under a pressure of 2 kg / cm for 60 minutes. After that, the reaction mixture was filtered.
    Regeneration solution. Carbonization. The filtrate from the stage of processing the ore sludge was pumped into a vessel for carbonization, the stirrer was turned on and the temperature was raised to 40 ° C,
    five
    five
    after that, uninterrupted streams of gaseous ammonia and carbon dioxide began to flow through the liquid, which were separated during the ore slurry processing stage. This reaction can be carried out in combination with the processing of ore sludge. Then, the reaction mixture was filtered, obtaining crystalline calcium carbonate as a filter residue, while the filtrate could be reused as a regenerated solution.
    The results of the experiment are presented in the table.
    Example 8. Phosphorus-containing ore from Mo Ping, Gui-Zhu Province, China.
    The chemical composition of the original ore,%: pentoxide 30,69; calcium oxide 48.41; magnesium oxide 2.82; ferric oxide 0.79; alumina 0.29.
    The implementation of the method. Processing of ore sludge. For the preparation of ore sludge, 1000 g of the original BOW powdered ore and 6000 g of a solution of mixed ammonium salts with a concentration of 14.5% were taken (with a weight ratio of ammonium chloride and ammonium nitrate of 5.6: 1), then the stock was loaded into the reaction vessel, included stirrer and increased the temperature to 180 C. The reaction was carried out under a pressure of 6 kg / cm for 30 minutes. Thereafter, the reaction mixture was filtered, obtaining phosphorus concentrate as a filter residue, while the filtrate and gaseous ammonia and carbon dioxide emitted during the reaction could be sent for further processing at the stage of solution regeneration.
    Regeneration solution. Carbonization. The filtrate from the stage of processing the ore slurry was pumped into a vessel for carbonization, the stirrer was turned on, the temperature was raised to, and continuous streams of gaseous ammonia and carbon dioxide were released through the liquid, which were released during the processing of the ore slurry. This reaction can be carried out in combination with the processing of ore sludge. After that, the reaction mixture was filtered to obtain crystalline calcium carbonate as a filter residue, while the solution
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    can be reused as a regenerated solution.
    The results of the experiment are presented in the table.
    Example 9. Phosphorus-containing ore was obtained from Tao-Ping in Hu Bei Province, China. The composition of the ore is the following,%: 17,14; CaO 50.80; MgO 1.10; 0.55; ACO3 0.83; SiO 7.41.
    1000 g of phosphorus-containing ore powder, having a particle size of 100 mesh, and 7500 g of a mixed solution of NH4C1 and in a weight ratio of 10: 1, having a concentration of 10%, were introduced into the reactor. The mixed ore suspension was stirred and heated to 186 C. The reaction was carried out under a pressure of 3.6 kg / cm for 40 minutes. After filtration, the resulting precipitate represented the phosphorus-containing concentrate as a product, the filtrate and the gases obtained in the reaction were introduced into the carbonization step.
    The filtrate was introduced into the carbonization reactor, stirred and heated to 40 ° C with the continuous introduction of gases (mainly NH and CO), resulting from the reaction in suspension, into the carbonization reactor to effect carbonization. The mixture was filtered. The precipitate contained mainly CaCOj, and the filtrate was a regenerated solution and could be used as a solution of the ammonium salt in the above-mentioned suspension reaction.
    The results are presented in the table.
    Example 10. Phosphorus-containing, ore was obtained from Salt Lake Or, its composition,%: 19,23; CaO 41.64; MgO 11.03; .0.34; 0.52; Si, 74.
    1000 g of ore powder having a particle size of 100 mesh and 4000 g of a mixed solution and in a weight ratio of 0.5: 1, having a concentration of 25%, were added to the reactor to form a reaction i slurry. This suspension was stirred and heated to 200 ° C. The reaction was conducted under a pressure of 4 kg / cm for 60 minutes. After filtration, the resulting OS -; .. the dock represented the phosphorus-containing concentrate as product, the filtrate and gases (mainly NH, and CO), obtained during the reaction, were introduced into the regeneration stage.
    1315
    This filtrate was introduced into the carbonization reactor, stirred and heated until the gases (mainly NHj and COj) obtained during the slurry reaction in the carbonization reactor were continuously fed in to carbonize. The resulting carbonation mixture was filtered. The filter cake contained CaCOj, and this filtrate was introduced into the alkalizing step.
    The filtrate was placed in an alkaline reactor, stirred and heated to 50 ° C. Then an aqueous solution of ammonia, having a concentration of 25%, was added to the reactor to bring the pH of the filtrate to 10-12, and the reaction was made alkaline for 30 minutes, so that Mg is precipitated from this solution.
    The pH value of the liquid phase was adjusted with acid, then this mixture was introduced into the reaction in suspension.
    where the ammonium salt was used as a solution.
    The results are presented in the table.
    The method of enrichment of phosphorus-containing ore, including its treatment with an aqueous solution of a mixture of inorganic compounds, followed by separation of the solid phase as a product from the liquid phase and the output of the resulting gases, in order to reduce phosphorus losses, are treated with a solution of chloride mixture and ammonium ammonium with a concentration of 10-25Z, taken in an amount that provides a mass ratio of phosphorus-containing ore and an aqueous solution of 1: 4.0-7.5 with 105-200 (Gu = mass ratio of ammonium chloride and ammonium nitrate in a mixture of 0.5 -10,0 :one,
    权利要求:
    Claims (1)
    [1]
    Claim
    A method of enriching a phosphorus-containing ore, including treating it with an aqueous solution of a mixture of inorganic compounds, followed by separating the solid phase in the form of a product from the liquid phase and removing the resulting gases, characterized in that, in order to reduce phosphorus losses, the treatment is carried out with a solution of a mixture of ammonium chloride and nitrate with a concentration of 10-25%, taken in an amount of 20 providing a mass ratio of phosphorus-containing ore 'and an aqueous solution of 1: 4.0-7.5 at 105-200 * C ~ and a mass ratio of ammonium chloride and ammonium nitrate in a mixture of 0.5 -10.0: 1.
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    同族专利:
    公开号 | 公开日
    US4793979A|1988-12-27|
    TNSN86047A1|1990-01-01|
    CN85100187A|1985-09-10|
    AU5538386A|1986-10-09|
    MA20658A1|1986-10-01|
    AU572388B2|1988-05-05|
    BR8601407A|1986-12-09|
    CN85100187B|1985-09-10|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    WO1997015693A1|1996-08-13|1997-05-01|Yalestown Corporation N.V.|Method of concentrating carbonate-containing phosphate raw material|
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    申请号 | 申请日 | 专利标题
    CN85100187A|CN85100187B|1985-04-01|1985-04-01|Process for chemcial separation of phosphate ore|
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